Ethyl Acetate → 1-{3-[2-(1-Benzothiophen-5-yl)ethoxy]propyl}-3-azetidinol citrate

HRID 7454

反応式

HRID 7454 の反応式
[S:1]1[C:5]2[CH:6]=[CH:7][C:8]([CH2:10][CH2:11][O:12][CH2:13][CH2:14][CH2:15][N:16]3[CH2:19][CH:18]([OH:20])[CH2:17]3)=[CH:9][C:4]=2[CH:3]=[CH:2]1.O.[C:22]([OH:34])(=[O:33])[CH2:23][C:24]([CH2:29][C:30]([OH:32])=[O:31])([C:26]([OH:28])=[O:27])[OH:25].C(OCC)(=O)C>C(O)C>[C:22]([OH:34])(=[O:33])[CH2:23][C:24]([CH2:29][C:30]([OH:32])=[O:31])([C:26]([OH:28])=[O:27])[OH:25].[S:1]1[C:5]2[CH:6]=[CH:7][C:8]([CH2:10][CH2:11][O:12][CH2:13][CH2:14][CH2:15][N:16]3[CH2:19][CH:18]([OH:20])[CH2:17]3)=[CH:9][C:4]=2[CH:3]=[CH:2]1

参加物

5

反応物 3

HCID 8857Ethyl Acetate2 回HCID 222302-Hydroxy-1,2,3-propanetricarboxylic acid hydrate (1:1)HCID 9901946Edonerpic

生成物 1

HCID 665884541-{3-[2-(1-Benzothiophen-5-yl)ethoxy]propyl}-3-azetidinol citrate収率 89.8%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

反応条件

温度
25 °C

実験手順

In 14.4 mL of ethanol was dissolved 10.0 g of 1-{3-[2-(1-benzothiophen-5-yl)ethoxy]propyl}-3-azetidinol, followed by adding thereto 7.21 g of citric acid monohydrate, and the resulting mixture was heated at 50° C. to effect dissolution. To the resulting solution were added 35 mL of ethyl acetate and 5.6 mL of ethanol at 50° C., and stirred at 25° C. The reaction mixture was heated at 40° C., after which ethyl acetate (45 mL) was added dropwise thereto and the resulting mixture was stirred at 40° C. for 10 minutes and then at 10 to 20° C. for 1 hour. The crystals precipitated were collected by filtration to obtain 14.9 g of 1-{3-[2-(1-benzothiophen-5-yl)ethoxy]propyl}-3-azetidinol citrate as colorless crystals.

後処理

  1. additionby adding
  2. dissolutiondissolution
  3. temperatureThe reaction mixture was heated at 40° C.
  4. stirringthe resulting mixture was stirred at 40° C. for 10 minutes
  5. customThe crystals precipitated
  6. filtrationwere collected by filtration

出典と根拠

ORDレコード
ord-a36078b27fbd4edfadf1e49381c9fdfa
出典データセット
uspto-grants-2006_08
特許番号
US07087594B2

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